反应 #409976

反应方程式

1-oxyl-4-hydroxy-2,2,6,6-tetramethylpiperidine

p-xylene

→

white solid

收率 59.0%

1-(4-Methylbenzyl)oxy-4-hydroxy-2,2,6,6-tetramethylpiperidine

收率 59.0%

反应条件

后处理

1. 1
   温度is heated
2. 2
   温度at reflux for 48 hours
3. 3
   过滤The reaction mixture is filtered
4. 4
   其他to remove 1,4-dihydroxy-2,2,6,6-tetramethylpiperidine
5. 5
   洗涤the filtrate is washed with 10 w/v % ascorbic acid (1×50 mL)
6. 6
   workup.DISTILLATIONdistilled water (2×50 mL)
7. 7
   干燥The organic phase is dried over anhydrous sodium sulfate
8. 8
   其他the volatiles are removed in vacuo
9. 9
   其他The residue is recrystallized from heptane

实验过程

A mixture of 8.60 g (0.05 mol) of 1-oxyl-4-hydroxy-2,2,6,6-tetramethylpiperidine and 106.17 g (1.0 mol) of p-xylene under a nitrogen atmosphere is heated at reflux for 48 hours. The reaction mixture is filtered to remove 1,4-dihydroxy-2,2,6,6-tetramethylpiperidine, and the filtrate is washed with 10 w/v % ascorbic acid (1×50 mL) and distilled water (2×50 mL). The organic phase is dried over anhydrous sodium sulfate and the volatiles are removed in vacuo. The residue is recrystallized from heptane to give 4.00 g (59% yield) of a white solid melting at 92.5-93° C.

来源